使用 N , N'-二 丁基 -N , N , N ', N' - N'- 四甲基-乙二胺四氢硼酸酯( BTMETB )或 轻度和非水条件, 可以轻松地从相应的烷基卤化物和酰基卤化物以高收率制备各种对称的二烷基二酰基和二酰基二硫化物。 N , N'- 二苄基 -N , N , N ', N'- 四甲基 硼酸四氢硼酸铵( BZTMETB )和元素硫。通过在室温下用硼氢化钠的碱性溶液处理相应的氯化季铵或溴化季铵,可以轻松制备季铵化硼氢化物。
PROCESS FOR PRODUCING POLYMER TERMINATED WITH OPTIONALLY PROTECTED FUNCTIONAL GROUP
申请人:KURARAY Co. LTD.
公开号:EP0704460A1
公开(公告)日:1996-04-03
A process for producing polymers having terminal functional group which may be protected, comprises polymerizing a radical-polymerizable monomer with a polymerization initiator comprising at least one member selected from the group (A) consisting of thio-S-carboxylic acids represented by the following general formula (1) and dithiocarboxylic acids represented by the following general formula (2) and at least one member selected from the group (B) consisting of polysulfides represented by the following general formula (3), polysulfides represented by the following general formula (4) and sulfoxides:
wherein R¹ represents a hydrocarbon group which may have a substituent including functional group;
wherein R² represents a hydrocarbon group which may have a substituent including functional group;
wherein R³ and R⁴ each represents a hydrocarbon group which may have a substituent including functional group and n is an integer of 2 or more; and
R⁵- (S)m- R⁶ (4)
wherein R⁵ and R⁶ each represents a hydrocarbon group having a functional group and m is an integer of 2 or more. This process can produce polymers with which functional groups have been introduced into one end or both ends thereof, irrespective of the rate of polymerization or the degree of polymerization of the polymer that forms.
The present invention relates to a process for preparing the telomerase inhibitor imetelstat using a 3 steps per cycle phase support bound process comprising the steps of deprotection of the 3′-amino group of the support-bound oligonucleotide, coupling with a 5′-phosphoramidite, and sulfurization with an acyl disulfide, characterized by the absence of an additional capping step in each cycle that is used to prevent unreacted 3′-amino oligonucleotide groups from reacting during subsequent cycles. Imetelstat has formula below.
A simple and general method for the synthesis of diacyl disulfides is reported. Sulfur is allowed to react with sodium hydroxide to give sodium disulfide at 65 degrees C under PTC, which can react with acyl halides to afford diacyl disulfides in good to excellent isolated yields. The effects of solvents and phase transfer catalysts are discussed.